CN110335819A - A kind of regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic - Google Patents
A kind of regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic Download PDFInfo
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
The present invention relates to a kind of regulation method based on two-dimension single layer Transition-metal dichalcogenide energy valley polarization characteristic, include the following steps: that (1) grows two-dimension single layer Transition-metal dichalcogenide using chemical vapour deposition technique in substrate；(2) two-dimentional feeromagnetic metal is prepared using mechanical stripping method；(3) by alignment transfer platform, by two-dimentional feeromagnetic metal, alignment is transferred on two-dimension single layer Transition-metal dichalcogenide, forms two-dimension single layer Transition-metal dichalcogenide-two dimension feeromagnetic metal heterojunction structure；The present invention forms heterojunction structure using two-dimentional ferromagnetic metallic material and two-dimension single layer Transition-metal dichalcogenide, flexibility, the atom level thin thickness feature of two-dimensional material can be given full play to, the problem of effectively preventing three-dimensional-two dimensional heterostructures of traditional ferromagnetic metallic material and two-dimensional material formation and destroying two-dimensional material self character, can be applied to the developmental research of ultra-thin microization and flexible spinning electron and energy valley electronic device etc..
Description
Technical field
The present invention relates to one kind based on two-dimension single layer Transition-metal dichalcogenide material and two-dimentional feeromagnetic metal hetero-junctions
Energy valley polarization characteristic regulate and control method.
Background technique
With the progress of science and technology, the electronic technology of charge based on electronics and spin two intrinsic degree of freedom manipulation and
Extensive development has been obtained in conjunction with the spintronics of magnetics and microelectronics.In recent years, with the rise of two-dimensional material, science
Family produces keen interest for the energy valley of Bloch Electron as the research of freedom degree in special symmetry crystalline material.It is single
Layer graphene has hexagonal crystallographic texture, and dirac cone point, that is, K and K ' of two non-equivalences on the Fermi surface of Brillouin zone leads to
Time-reversal symmetry is crossed to connect each other.The Niu Qian group of texas,U.S university theoretically proposes by breaking the anti-of graphene
Symmetry is drilled, band gap occurs at two dirac cones, it will Quantum Transport behavior and the selection of energy valley circular-dichroism occurs
Absorbability realizes energy valley polarization and its measurement.However, controllable staggeredly lattice gesture is extremely difficult on laboratory in graphene
It realizes, the lattice symmetry for breaking graphene has huge challenge.
Transition-metal dichalcogenide is similar with graphene, is connected with each other in layer according to strength covalent bond, between layers
It is connected with each other by weak Van der Waals force, band gap is gradually increased as the number of plies is reduced, and when single layer is changed into direct band gap, and this
A little direct band gaps are alternately distributed the place non-equivalence energy valley K and K ' on the corner of Brillouin zone six.In addition, single layer Transition Metal Sulfur
Compounds of group has the honeycomb crystal lattice similar with graphene, and inversion symmetry is broken to be lacked.Therefore, they are that research can paddy electricity
The ideal natural material that son is learned.Due to the strong Quantum geometrical phase of transition metal atoms d track, the valence band on K and K ' energy valley is deposited
In biggish Spin Splitting, about 0.1-0.4eV；On the other hand, since Time-reversal symmetry determines the K and K ' of non-equivalence
Spin Splitting in energy valley is necessarily opposite.This spin-energy valley coupling physical mechanism makes the interband of different energy valleys (K/K ')
Optical transition can be by the photon excitation of different polarization (left-hand/right-hand).By controlling the circular polarization of excitation light source, Ke Yishi
Now stable energy valley polarizing control and the interaction regulation to spin and energy valley freedom degree.
By to the polarized stability contorting of energy valley, using energy valley freedom degree as information carrier, may be implemented a kind of new
Coding mode information, such as: two different energy valley K and K ' can be respectively corresponded two kinds of logic states " 0 " and " 1 " Lai Jinhang
The storage of data.It is this by regulating and controlling energy valley freedom degree to design and Implement correlation function compared with traditional electronic component
Device has many advantages, such as that information is not easy to lose, processing speed is fast, low in energy consumption, integrated level is high.In conjunction with material itself electricity and
Optical characteristics may be implemented the functions such as storage, logic and communication are highly integrated based on electronics energy valley freedom degree
Novel and multifunctional quantum device.It realizes although having been reported through the conventional antiferromagnetics such as MnO, CoO material to single layer transition gold
The energy valley polarization characteristic for belonging to chalcogenide is regulated and controled, but because these conventional antiferromagnetic materials are body material, with single layer
The hetero-junctions that Transition-metal dichalcogenide is formed cannot give full play to two-dimensional material itself atomic-level thickness and flexible excellent
Anisotropic energy.
Summary of the invention
In order to give full play to excellent properties of the two-dimensional material in the regulation of energy valley polarization characteristic, the present invention provides a kind of benefits
Energy valley polarization is carried out with two-dimension single layer Transition-metal dichalcogenide with the heterojunction structure that two-dimentional feeromagnetic metal couples hydridization formation
The new method of characteristic regulation grows two-dimension single layer Transition-metal dichalcogenide material, machinery stripping using chemical vapour deposition technique
Generate two-dimentional feeromagnetic metal from method, using neighbour's magnetic moment coupling effect, by adjusting hetero-junctions way of stacking to energy valley polarize into
Row regulation.
The technical solution adopted by the present invention is that:
A kind of regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic, includes the following steps:
(1) two-dimension single layer Transition-metal dichalcogenide is grown in substrate using chemical vapour deposition technique；
(2) two-dimentional feeromagnetic metal is prepared using mechanical stripping method；
(3) by alignment transfer platform, by two-dimentional feeromagnetic metal, alignment is transferred to two-dimension single layer transition metal sulfur family chemical combination
On object, two-dimension single layer Transition-metal dichalcogenide-two dimension feeromagnetic metal heterojunction structure is formed；Angle when by alignment transfer
Degree control realizes way of stacking different between two-dimension single layer Transition-metal dichalcogenide and two-dimentional feeromagnetic metal, with regulation
The energy valley polarization characteristic of two-dimension single layer Transition-metal dichalcogenide.
Preferably, the Transition-metal dichalcogenide molecular formula is MX2, M=Mo or W, X=S or Se.
Preferably, the Transition-metal dichalcogenide is tungsten disulfide, and step (1) is specifically: using tungstic acid
With sulphur powder as chemical vapour deposition reaction source, substrate is tipped upside down on to the quartz for being placed in reaction chamber middle storage tungstic acid
On boat, sulphur powder, which is placed in quartz boat, to be placed at reaction chamber uptake, is controlled reaction temperature and reaction time, is grown in substrate
Deposition forms tungsten disulfide film.
Preferably, the substrate is SiO2/ Si substrate.
Preferably, the substrate is prepared with the following method: by SiO2/ Si substrate is rinsed with a large amount of deionized waters, first
After be put into acetone soln, ethanol solution and deionized water solution 5~10min of ultrasonic cleaning, cleaning is completed to take out three times
Substrate is dried up using inert gas.
Preferably, the inert gas is nitrogen.
Preferably, step (2) is specifically: the ferromagnetic gold of lower two dimension is removed from feeromagnetic metal crystal using high transparency adhesive tape is thought
Belong to, by adhesive tape repeatedly to gluing 5~8 times, obtains two-dimentional feeromagnetic metal thin layer；Then the clean load for being stained with PDMS is adhered to
On slide, adhesive tape is taken off after slight squeeze 3~5 is lower.
Preferably, the feeromagnetic metal is MnB2Or FeB2Or CrB2。
Preferably, step (3) is specifically: will grow the SiO for having single layer two dimension Transition-metal dichalcogenide2/ Si base
Piece is placed on alignment transfer platform objective table, and by being directed at transfer station, obtained two-dimentional feeromagnetic metal thin layer/PDMS/ is carried
Slide attaches on single layer two dimension Transition-metal dichalcogenide, squeezes intermediate air, make two-dimentional feeromagnetic metal thin layer and
Single layer two dimension Transition-metal dichalcogenide is pasted completely keeps 10~20min；Sample is placed on warm table, at 60~80 DEG C
After 10~30min of lower heating, lower SiO is prized with tweezers low force2/ Si substrate makes hetero-junctions be detached from and be attached on PDMS/ glass slide
SiO2On/Si substrate；Angles and positions control when by alignment transfer platform adherency, can be obtained the two dimension of different way of stacking
Single layer Transition-metal dichalcogenide-two dimension feeromagnetic metal heterojunction structure.
In order to preferably grow surface uniformity, the good two-dimension single layer Transition-metal dichalcogenide of continuity is thin
Film, to obtain two-dimension single layer Transition-metal dichalcogenide-two dimension feeromagnetic metal heterojunction structure, it is preferable that step (1) is specific
It is:
(a) first by SiO2/ Si substrate is cleaned with deionized water, then in acetone soln ultrasonic cleaning 5~
10min, takes out substrate and is cleaned by ultrasonic 5~10min in being put into ethanol solution, takes out substrate again and is put into deionized water
5~10min is cleaned, the SiO2/Si substrate that cleaning is completed is with being dried with nitrogen；
(b) by SiO2/ Si substrate and tungstic acid or molybdenum trioxide target source material are respectively put into thermal evaporation plated film instrument chamber
On indoor luggage carrier and in crucible, chamber is evacuated to 10-4Pa using pumped vacuum systems, the target source in heating crucible
Material escapes its molecule from surface to form steam stream and deposit to SiO2/ Si substrate surface, the raw material for forming 1~5nm thickness are thin
Film；
(c) it using pumped vacuum systems by pipe reaction stove evacuation to 10-2Torr, and is purged with the argon gas of 200sccm
To normal pressure state, source material film/SiO of 0.5~10nm thickness will be deposited2/ Si substrate, which is put into quartz boat, to be placed in
Then the SiO2/Si substrate for growing two-dimensional material is buckled in this substrate by the heating zone center of tube furnace reaction chamber
Side is kept between the two away from less than 1mm；
(d) it weighs 200mg sulphur powder or selenium powder is put into quartz boat and is placed at the uptake of reaction chamber, and in (c)
The distance between quartz boat is maintained between 10~20cm；
(e) it is maintained at the temperature of tube furnace reaction chamber central area between 600~950 DEG C by heating coil, sulphur
Or the temperature of selenium source is maintained between 150~300 DEG C；Keep argon stream amount between 10~150sccm, growth time 5
~60min；After growth is completed, heating coil is closed, is naturally cooling to room temperature in an argon atmosphere, takes out sample.
The beneficial effects of the present invention are:
1, the present invention forms heterojunction structure using two-dimentional ferromagnetic metallic material and two-dimension single layer Transition-metal dichalcogenide,
Flexibility, the atom level thin thickness feature that two-dimensional material can be given full play to effectively prevent traditional ferromagnetic metallic material and two dimension
Three-dimensional-two dimensional heterostructures that material is formed and the problem of destroy two-dimensional material self character, can be applied to ultra-thin microization and
The developmental research of flexible spinning electron and energy valley electronic device etc.；
2, the present invention can pass through two-dimentional ferromagnetic metallic material-two-dimension single layer Transition-metal dichalcogenide hetero-junctions
Different way of stacking regulate and control the splitting energy of K and K ' energy valley；
3, mechanical stripping method of the present invention is at low cost, easy to operate, chemical vapour deposition technique have controllability it is good,
The advantages of growing single layer two dimension Transition-metal dichalcogenide film uniformity.
Detailed description of the invention
Fig. 1 is six kinds of two-dimentional ferromagnetic metallic material-two-dimension single layer Transition-metal dichalcogenide hetero-junctions typical stackings
Schematic diagram；
Fig. 2 is six kinds of two-dimentional ferromagnetic metallic material-two-dimension single layer Transition-metal dichalcogenide hetero-junctions typical stackings
Implementation schematic diagram；
Fig. 3 is six kinds of typical stacking two dimension ferromagnetic metallic materials-two-dimension single layer transition gold when considering Quantum geometrical phase
Belong to the spin projection energy band diagram of two-dimension single layer Transition-metal dichalcogenide in chalcogenide hetero-junctions.
Specific embodiment
The present invention is further explained in the light of specific embodiments, but invention which is intended to be protected and unlimited
In this.
Embodiment 1
A kind of regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic, includes the following steps:
(1) MnB is prepared first2- WS2Single layer WS in heterojunction structure2Material:
Tube furnace reaction chamber is evacuated to 10- 2Torr is purged with 200sccm argon gas to recovery normal pressure state.
Prepare two pieces of SiO2/ Si substrate A and B, by two pieces of SiO2/ Si substrate is rinsed with a large amount of deionized waters, and it is molten to be put into acetone
It is cleaned by ultrasonic 8min in liquid, takes out substrate, be put into ethanol solution and be cleaned by ultrasonic 8min, take out substrate again, be put into
It is cleaned by ultrasonic 8min in ionized water, cleaned substrate is dried up with inert nitrogen gas.
By SiO2/ Si substrate A is put on the indoor luggage carrier of thermal evaporation plated film instrument chamber, and tungsten trioxide powder is put into thermal evaporation
In the indoor crucible of plated film instrument chamber, chamber is evacuated to 10 using pumped vacuum systems- 4Pa, the tungstic acid in heating crucible
Powder escapes its molecule from surface vaporization, forms steam stream, deposits to SiO2The surface /Si substrate A forms the uniform of 5nm thickness
WO 3 film.
The SiO of 5nm thickness WO 3 film will be deposited2/ Si substrate A is placed in quartz boat that be placed in tube furnace anti-
The heating zone centre for answering chamber, then by SiO2/ Si substrate B is tipped upside down on above A substrate, is kept between the two away from less than 1mm.
Weigh 200mg sulphur powder to be put into quartz boat, be placed at the uptake of reaction chamber, keep and tungsten source between away from
From for 15cm.
The temperature that tungsten source is kept by the heating coil of tube furnace reaction chamber is 900 DEG C, and sulphur source temperature is 200 DEG C.It protects
The argon stream being passed through is held in 100sccm, growth time 30min.Growth closes heating coil and in argon atmospher after completing
It is naturally cooling to room temperature in enclosing, takes out sample, obtains single layer WS2Material.
(2) MnB is then prepared2- WS2MnB in heterojunction structure2Material:
MnB is attached to using the think of high transparency adhesive tape of tweezers clamping 10cm length2Plane of crystal is gently compacted, and makes adhesive tape
And MnB2It slowly tears after tightly attaching.Then by the doubling of adhesive tape both ends, make MnB2Thin slice, which is clipped in adhesive tape, to be had in sticky side
Between, it slowly tears after being gently compacted.It removes 6 times repeatedly, just has MnB on adhesive tape2Thin slice.Then it is adhered to and has been glued
On clean slide with PDMS, adhesive tape is taken off after slight squeeze 5 is lower, obtains MnB2Thin slice/PDMS/ glass slide.
(3) will finally grow has single layer WS2SiO2/ Si substrate is placed on alignment transfer platform objective table, by right
Quasi- transfer platform slowly reduces MnB2/ PDMS/ glass slide height simultaneously controls its position and angle, is attached to WS2/SiO2/Si
On substrate and intermediate air is squeezed, makes MnB2And WS2It is attached after keeping 15min completely, sample is placed on warm table,
After heating 20min at 70 DEG C, lower SiO is prized with tweezers low force2/ Si substrate makes hetero-junctions be detached from and be attached on PDMS/ glass slide
SiO2On/Si substrate, MnB is obtained2- WS2Heterojunction structure.
Referring to Figures 1 and 2, by taking side length is the equilateral triangle sample of d as an example, material 1 is two-dimension single layer transition metal sulfur family
Compound, material 2 are two-dimentional feeromagnetic metal.During material 2 is transferred to material 1 with alignment transfer platform, two kinds of materials
Stacking 1 can be achieved after expecting 0 ° of aligned stack；2 relative material 1 of material translates up d/12, then to right translation d/6, last counterclockwise
Stacking 2 can be achieved in 60 ° of rotation after aligned stack；2 60 ° of the rotation counterclockwise of relative material 1 of material, can be achieved heap after aligned stack
Pile 3；2 relative material 1 of material translates d/12 still further below, stacking 4 can be achieved after aligned stack to right translation d/12；Material 2 is opposite
Material 1 is to left d/12, then translates up d/12, and stacking 5 can be achieved after aligned stack；2 relative material 1 of material is to right translation
D/12 translates d/12 still further below, and stacking 6 can be achieved in last 60 ° of rotation counterclockwise after aligned stack.
Referring to Fig. 3, pass through two-dimentional ferromagnetic metallic material-two-dimension single layer transition metal sulfur family chemical combination of six kinds of typical stackings
Object hetero-junctions construction, two-dimension single layer Transition-metal dichalcogenide respectively can be 115.5 in the valence band splitting energy of K and K ' energy valley
Regulation, while the energy valley point of the first and second valence band after division are realized within the scope of~560.0meV and 112.3~559.0meV
Regulation can be realized within the scope of 21.3~253.0meV and 20.8~194.3meV by splitting difference.
Tungsten source employed in the present embodiment and sulphur source purity are 99.9% or more, the SiO of selection2/ Si substrate surface
Smooth and oxidated layer thickness is 285nm.
Embodiment 2
A kind of regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic, includes the following steps:
(1) FeB is prepared first2- WS2WS in heterojunction structure2Monolayer material:
Tube furnace reaction chamber is evacuated to 10- 2Torr is purged with 200sccm argon gas to recovery normal pressure state.
Prepare two pieces of SiO2/ Si substrate A and B, by two pieces of SiO2/ Si substrate is rinsed with a large amount of deionized waters, and it is molten to be put into acetone
It is cleaned by ultrasonic 8min in liquid, takes out substrate, be put into ethanol solution and be cleaned by ultrasonic 8min, take out substrate again, be put into
It is cleaned by ultrasonic 8min in ionized water, cleaned substrate is dried up with inert nitrogen gas.
By SiO2/ Si substrate A is put on the indoor luggage carrier of thermal evaporation plated film instrument chamber, and tungsten trioxide powder is put into thermal evaporation
In the indoor crucible of plated film instrument chamber, chamber is evacuated to 10 using pumped vacuum systems- 4Pa, the tungstic acid in heating crucible
Powder escapes its molecule from surface vaporization, forms steam stream, deposits to SiO2The surface /Si substrate A forms the uniform of 5nm thickness
WO 3 film.
The SiO of 5nm thickness WO 3 film will be deposited2/ Si substrate A is placed in quartz boat that be placed in tube furnace anti-
The heating zone centre for answering chamber, then by SiO2/ Si substrate B is tipped upside down on above A substrate, is kept between the two away from less than 1mm.
Weigh 200mg sulphur powder to be put into quartz boat, be placed at the uptake of reaction chamber, keep and tungsten source between away from
From for 15cm.
The temperature that tungsten source is kept by the heating coil of tube furnace reaction chamber is 900 DEG C, and sulphur source temperature is 200 DEG C.It protects
The argon stream being passed through is held in 100sccm, growth time 30min, growth closes heating coil and in argon atmospher after completing
It is naturally cooling to room temperature in enclosing, takes out sample, obtains single layer WS2Material.
(2) FeB is then prepared2- WS2FeB in heterojunction structure2Material:
FeB is attached to using the think of high transparency adhesive tape of tweezers clamping 10cm length2Plane of crystal is gently compacted, and makes adhesive tape
And FeB2It slowly tears after tightly attaching.Then by the doubling of adhesive tape both ends, make FeB2Thin slice, which is clipped in adhesive tape, to be had in sticky side
Between, it slowly tears after being gently compacted.It removes 6 times repeatedly, just has FeB on adhesive tape2Thin slice.Then it is adhered to and has been glued
On clean slide with PDMS, adhesive tape is taken off after slight squeeze 5 is lower, obtains FeB2Thin slice/PDMS/ glass slide.
(3) will finally grow has single layer WS2SiO2/ Si substrate is placed on alignment transfer platform objective table, by right
Quasi- transfer platform slowly reduces FeB2/ PDMS/ glass slide height simultaneously controls its position and angle, is attached to WS2/SiO2/Si
On substrate and intermediate air is squeezed, makes FeB2And WS2It is attached after keeping 15min completely, sample is placed on warm table,
After heating 20min at 70 DEG C, lower SiO is prized with tweezers low force2/ Si substrate makes hetero-junctions be detached from and be attached on PDMS/ glass slide
SiO2On/Si substrate, FeB is obtained2- WS2Heterojunction structure.
Tungsten source employed in the present embodiment and sulphur source purity are 99.9% or more, the SiO of selection2/ Si substrate surface
Smooth and oxidated layer thickness is 285nm.
Embodiment 3
A kind of regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic, includes the following steps:
(1) CrB is prepared first2- WS2WS in heterojunction structure2Monolayer material:
Tube furnace reaction chamber is evacuated to 10- 2Torr is purged with 200sccm argon gas to recovery normal pressure state.
Prepare two pieces of SiO2/ Si substrate A and B, by two pieces of SiO2/ Si substrate is rinsed with a large amount of deionized waters, and it is molten to be put into acetone
It is cleaned by ultrasonic 8min in liquid, takes out substrate, be put into ethanol solution and be cleaned by ultrasonic 8min, take out substrate again, be put into
It is cleaned by ultrasonic 8min in ionized water, cleaned substrate is dried up with inert nitrogen gas.
By SiO2/ Si substrate A is put on the indoor luggage carrier of thermal evaporation plated film instrument chamber, and tungsten trioxide powder is put into thermal evaporation
In the indoor crucible of plated film instrument chamber, chamber is evacuated to 10 using pumped vacuum systems- 4Pa, the tungstic acid in heating crucible
Powder escapes its molecule from surface vaporization, forms steam stream, deposits to SiO2The surface /Si substrate A forms the uniform of 5nm thickness
WO 3 film.
The SiO of 5nm thickness WO 3 film will be deposited2/ Si substrate A is placed in quartz boat that be placed in tube furnace anti-
The heating zone centre for answering chamber, then by SiO2/ Si substrate B is tipped upside down on above A substrate, is kept between the two away from less than 1mm.
Weigh 200mg sulphur powder to be put into quartz boat, be placed at the uptake of reaction chamber, keep and tungsten source between away from
From for 15cm.
The temperature that tungsten source is kept by the heating coil of tube furnace reaction chamber is 900 DEG C, and sulphur source temperature is 200 DEG C.It protects
The argon stream being passed through is held in 100sccm, growth time 30min, growth closes heating coil and in argon atmospher after completing
It is naturally cooling to room temperature in enclosing, takes out sample, obtains single layer WS2Material.
(2) CrB is then prepared2- WS2CrB in heterojunction structure2Material:
CrB is attached to using the think of high transparency adhesive tape of tweezers clamping 10cm length2Plane of crystal is gently compacted, and makes adhesive tape
And CrB2It slowly tears after tightly attaching.Then by the doubling of adhesive tape both ends, make CrB2Thin slice, which is clipped in adhesive tape, to be had in sticky side
Between, it slowly tears after being gently compacted.It removes 6 times repeatedly, just has CrB on adhesive tape2Thin slice.Then it is adhered to and has been glued
On clean slide with PDMS, adhesive tape is taken off after slight squeeze 5 is lower, obtains CrB2Thin slice/PDMS/ glass slide.
(3) will finally grow has WS2SiO2/ Si substrate is placed on alignment transfer platform objective table, is turned by alignment
Moving platform slowly reduces CrB2/ PDMS/ glass slide height simultaneously controls its position and angle, is attached to WS2/SiO2/ Si substrate
Air that is upper and squeezing centre, makes CrB2And WS2It attaches after keeping 15min, sample is placed on warm table, at 70 DEG C completely
After lower heating 20min, lower SiO is prized with tweezers low force2/ Si substrate makes hetero-junctions and PDMS/ glass slide be detached from and be attached on SiO2/
On Si substrate, CrB is obtained2- WS2Heterojunction structure.
Tungsten source employed in the present embodiment and sulphur source purity are 99.9% or more, the SiO of selection2/ Si substrate surface
Smooth and oxidated layer thickness is 285nm.
Embodiment 4
A kind of regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic, includes the following steps:
(1) MnB is prepared first2- MoS2MoS in heterojunction structure2Monolayer material:
Tube furnace reaction chamber is evacuated to 10- 2Torr is purged with 200sccm argon gas to recovery normal pressure state.
Prepare two pieces of SiO2/ Si substrate A and B, by two pieces of SiO2/ Si substrate is rinsed with a large amount of deionized waters, and it is molten to be put into acetone
It is cleaned by ultrasonic 8min in liquid, takes out substrate, be put into ethanol solution and be cleaned by ultrasonic 8min, take out substrate again, be put into
It is cleaned by ultrasonic 8min in ionized water, cleaned substrate is dried up with inert nitrogen gas.
By SiO2/ Si substrate A is put on the indoor luggage carrier of thermal evaporation plated film instrument chamber, and molybdenum trioxide powder is put into thermal evaporation
In the indoor crucible of plated film instrument chamber, chamber is evacuated to 10 using pumped vacuum systems- 4Pa, the molybdenum trioxide in heating crucible
Powder escapes its molecule from surface vaporization, forms steam stream, deposits to SiO2The surface /Si substrate A forms the uniform of 5nm thickness
Molybdenum Oxide Thin Films by Sol-Gel.
The SiO of 5nm thickness Molybdenum Oxide Thin Films by Sol-Gel will be deposited2/ Si substrate A is placed in quartz boat that be placed in tube furnace anti-
The heating zone centre for answering chamber, then by SiO2/ Si substrate B is tipped upside down on above A substrate, is kept between the two away from less than 1mm.
Weigh 200mg sulphur powder to be put into quartz boat, be placed at the uptake of reaction chamber, keep and molybdenum source between away from
From for 18cm.
The temperature that molybdenum source is kept by the heating coil of pipe reaction chamber is 800 DEG C, and sulphur source temperature is 200 DEG C.It keeps
The argon stream being passed through in 100sccm, growth time 30min, close heating coil and in argon atmosphere after completing by growth
In be naturally cooling to room temperature, take out sample, obtain MoS2Monolayer material.
(2) MnB is then prepared2- MoS2MnB in heterojunction structure2Material:
MnB is attached to using the think of high transparency adhesive tape of tweezers clamping 10cm length2Plane of crystal is gently compacted, and makes adhesive tape
And MnB2It slowly tears after tightly attaching.Then by the doubling of adhesive tape both ends, make MnB2Thin slice, which is clipped in adhesive tape, to be had in sticky side
Between, it slowly tears after being gently compacted.It removes 6 times repeatedly, just has MnB on adhesive tape2Thin slice.Then it is adhered to and has been glued
On clean slide with PDMS, adhesive tape is taken off after slight squeeze 5 is lower, obtains MnB2Thin slice/PDMS/ glass slide.
(3) will finally grow has MoS2SiO2/ Si substrate is placed on alignment transfer platform objective table, passes through alignment
Transfer platform slowly reduces MnB2/ PDMS/ glass slide height simultaneously controls its position and angle, is attached to MoS2/SiO2/Si
On substrate and intermediate air is squeezed, makes MnB2And WS2It is attached after keeping 15min completely, sample is placed on warm table,
After heating 20min at 75 DEG C, lower SiO is prized with tweezers low force2/ Si substrate makes hetero-junctions be detached from and be attached on PDMS/ glass slide
SiO2On/Si substrate, MnB is obtained2- MoS2Heterojunction structure.
Molybdenum source employed in the present embodiment and sulphur source purity are 99.9% or more, the SiO of selection2/ Si substrate surface
Smooth and oxidated layer thickness is 285nm.
Embodiment 5
A kind of regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic, includes the following steps:
(1) FeB is prepared first2- MoS2MoS in heterojunction structure2Thin-film material:
Tube furnace reaction chamber is evacuated to 10- 2Torr is purged with 200sccm argon gas to recovery normal pressure state.
Prepare two pieces of SiO2/ Si substrate A and B, by two pieces of SiO2/ Si substrate is rinsed with a large amount of deionized waters, and it is molten to be put into acetone
It is cleaned by ultrasonic 8min in liquid, takes out substrate, be put into ethanol solution and be cleaned by ultrasonic 8min, take out substrate again, be put into
It is cleaned by ultrasonic 8min in ionized water, cleaned substrate is dried up with inert nitrogen gas.
By SiO2/ Si substrate A is put on the indoor luggage carrier of thermal evaporation plated film instrument chamber, and molybdenum trioxide powder is put into thermal evaporation
In the indoor crucible of plated film instrument chamber, chamber is evacuated to 10 using pumped vacuum systems- 4Pa, the molybdenum trioxide in heating crucible
Powder escapes its molecule from surface vaporization, forms steam stream, deposits to SiO2The surface /Si substrate A forms the equal of 5nm thickness
Even Molybdenum Oxide Thin Films by Sol-Gel.
The SiO of 5nm thickness Molybdenum Oxide Thin Films by Sol-Gel will be deposited2/ Si substrate A, which is placed in quartz boat, is placed in tube furnace
The heating zone centre of reaction chamber, then by SiO2/ Si substrate B is tipped upside down on above A substrate, is kept between the two away from less than 1mm.
Weigh 200mg sulphur powder to be put into quartz boat, be placed at the uptake of reaction chamber, keep and molybdenum source between away from
From for 18cm.
The temperature that molybdenum source is kept by the heating coil of tube furnace reaction chamber is 800 DEG C, and sulphur source temperature is 200 DEG C.It protects
The argon stream being passed through is held in 10sccm, growth time 30min, growth closes heating coil and in argon atmosphere after completing
In be naturally cooling to room temperature, take out sample, obtain MoS2Monolayer material.
(2) FeB is then prepared2- MoS2FeB in heterojunction structure2Material:
FeB is attached to using the think of high transparency adhesive tape of tweezers clamping 10cm length2Plane of crystal is gently compacted, and makes adhesive tape
And FeB2It slowly tears after tightly attaching.Then by the doubling of adhesive tape both ends, make FeB2Thin slice, which is clipped in adhesive tape, to be had in sticky side
Between, it slowly tears after being gently compacted.It removes 6 times repeatedly.Just has FeB on adhesive tape2Thin slice.Then it is adhered to and has been glued
On clean slide with PDMS, adhesive tape is taken off after slight squeeze 5 is lower, obtains FeB2Thin slice/PDMS/ glass slide.
(3) will finally grow has MoS2SiO2/ Si substrate is placed on alignment transfer platform objective table, passes through alignment
Transfer platform slowly reduces FeB2/ PDMS/ glass slide height simultaneously controls its position and angle, is attached to MoS2/SiO2/Si
On substrate and intermediate air is squeezed, makes FeB2And WS2It is attached after keeping 15min completely, sample is placed on warm table,
After heating 20min at 70 DEG C, lower SiO is prized with tweezers low force2/ Si substrate makes hetero-junctions be detached from and be attached on PDMS/ glass slide
SiO2On/Si substrate, FeB is obtained2- MoS2Heterojunction structure.
Molybdenum source employed in the present embodiment and sulphur source purity are 99.9% or more, the SiO of selection2/ Si substrate surface
Smooth and oxidated layer thickness is 285nm.
Embodiment 6
A kind of regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic, includes the following steps:
(1) CrB is prepared first2- MoS2MoS in heterojunction structure2Thin-film material:
Tube furnace reaction chamber is evacuated to 10- 2Torr is purged with 200sccm argon gas to recovery normal pressure state.
Prepare two pieces of SiO2/ Si substrate A and B, by two pieces of SiO2/ Si substrate is rinsed with a large amount of deionized waters, and it is molten to be put into acetone
It is cleaned by ultrasonic 8min in liquid, takes out substrate, be put into ethanol solution and be cleaned by ultrasonic 8min, take out substrate again, be put into
It is cleaned by ultrasonic 8min in ionized water, cleaned substrate is dried up with inert nitrogen gas.
By SiO2/ Si substrate A is put on the indoor luggage carrier of thermal evaporation plated film instrument chamber, and molybdenum trioxide powder is put into thermal evaporation
In the indoor crucible of plated film instrument chamber, chamber is evacuated to 10 using pumped vacuum systems- 4Pa, the molybdenum trioxide in heating crucible
Powder escapes its molecule from surface vaporization, forms steam stream, deposits to SiO2The surface /Si substrate A forms the equal of 5nm thickness
Even Molybdenum Oxide Thin Films by Sol-Gel.
The SiO of 5nm thickness Molybdenum Oxide Thin Films by Sol-Gel will be deposited2/ Si substrate A, which is placed in quartz boat, is placed in tube furnace
The heating zone centre of reaction chamber, then by SiO2/ Si substrate B is tipped upside down on above A substrate, is kept between the two away from less than 1mm.
Weigh 200mg sulphur powder to be put into quartz boat, be placed at the uptake of reaction chamber, keep and molybdenum source between away from
From for 18cm.
The temperature that molybdenum source is kept by the heating coil of tube furnace reaction chamber is 800 DEG C, and sulphur source temperature is 200 DEG C.It protects
The argon stream being passed through is held in 100sccm, growth time 30min, growth closes heating coil and in argon atmospher after completing
It is naturally cooling to room temperature in enclosing, takes out sample, obtains MoS2Monolayer material.
(2) CrB is then prepared2- MoS2Cr in heterojunction structure2B thin-film material:
CrB is attached to using the special adhesive tape that the mechanical stripping method of tweezers clamping 10cm length uses2Plane of crystal, gently
Compacting, makes adhesive tape and CrB2It slowly tears after tightly attaching.Then by the doubling of adhesive tape both ends, make CrB2Thin slice, which is clipped in adhesive tape, to be had
The centre of sticky side is slowly torn after being gently compacted.It removes 6 times repeatedly, just has CrB on adhesive tape2Thin slice.Then
It is adhered to and has been stained on the clean slide of PDMS, taken adhesive tape off after slight squeeze 5 is lower, obtain CrB2Thin slice/PDMS/ is carried
Slide.
(3) will finally grow has single layer MoS2SiO2/ Si substrate is placed on alignment transfer platform objective table, is passed through
Alignment transfer platform slowly reduces CrB2/ PDMS/ glass slide height simultaneously controls its position and angle, is attached to MoS2/
SiO2On/Si substrate and intermediate air is squeezed, makes CrB2And WS2It is attached after keeping 15min completely, sample is placed and is heated
On platform, after heating 20min at 75 DEG C, lower SiO is prized with tweezers low force2/ Si substrate is detached from hetero-junctions and PDMS/ glass slide
And it is attached on SiO2On/Si substrate, CrB is obtained2- MoS2Heterojunction structure.
Molybdenum source employed in the present embodiment and sulphur source purity are 99.9% or more, the SiO of selection2/ Si substrate surface
Smooth and oxidated layer thickness is 285nm.
Embodiment 7
A kind of regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic, includes the following steps:
(1) MnB is prepared first2- WSe2WSe in heterojunction structure2Monolayer material:
Tube furnace reaction chamber is evacuated to 10- 2Torr is purged with 200sccm argon gas to recovery normal pressure state.
Prepare two pieces of SiO2/ Si substrate A and B, by two pieces of SiO2/ Si substrate is rinsed with a large amount of deionized waters, and it is molten to be put into acetone
It is cleaned by ultrasonic 8min in liquid, takes out substrate, be put into ethanol solution and be cleaned by ultrasonic 8min, take out substrate again, be put into
It is cleaned by ultrasonic 8min in ionized water, cleaned substrate is dried up with inert nitrogen gas.
By SiO2/ Si substrate A is put on the indoor luggage carrier of thermal evaporation plated film instrument chamber, and tungsten trioxide powder is put into thermal evaporation
In the indoor crucible of plated film instrument chamber, chamber is evacuated to 10 using pumped vacuum systems- 4Pa, the tungstic acid in heating crucible
Powder escapes its molecule from surface vaporization, forms steam stream, deposits to SiO2The surface /Si substrate A forms the uniform of 5nm thickness
WO 3 film.
The SiO of 5nm thickness WO 3 film will be deposited2/ Si substrate A is placed in quartz boat that be placed in tube furnace anti-
The heating zone centre for answering chamber, then by SiO2/ Si substrate B is tipped upside down on above A substrate, is kept between the two away from less than 1mm.
Weigh 200mg selenium powder to be put into quartz boat, be placed at the uptake of reaction chamber, keep and tungsten source between away from
From for 15cm.
The temperature that tungsten source is kept by the heating coil of tube furnace reaction chamber is 900 DEG C, and selenium source temperature is 200 DEG C.It protects
The argon stream being passed through is held in 100sccm, growth time 30min, growth closes heating coil and in argon atmospher after completing
It is naturally cooling to room temperature in enclosing, takes out sample, obtains single layer WSe2Material.
(2) MnB is then prepared2- WSe2MnB in heterojunction structure2Material:
MnB is attached to using the think of high transparency adhesive tape of tweezers clamping 13cm length2Plane of crystal is gently compacted, and makes adhesive tape
And WSe2It slowly tears after tightly attaching.Then by the doubling of adhesive tape both ends, make MnB2Thin slice, which is clipped in adhesive tape, to be had in sticky side
Between, it slowly tears after being gently compacted.It removes 6 times repeatedly, just has MnB on adhesive tape2Thin slice.Then it is adhered to and has been glued
On clean slide with PDMS, adhesive tape is taken off after slight squeeze 5 is lower, obtains MnB2Thin slice/PDMS/ glass slide.
(3) will finally grow has single layer WSe2SiO2/ Si substrate is placed on alignment transfer platform objective table, is passed through
Alignment transfer platform slowly reduces MnB2/ PDMS/ glass slide height simultaneously controls its position and angle, is attached to WSe2/
SiO2On/Si substrate and intermediate air is squeezed, makes MnB2And WSe2It is attached after keeping 15min completely, sample is placed and is heated
On platform, after heating 20min at 70 DEG C, lower SiO is prized with tweezers low force2/ Si substrate is detached from hetero-junctions and PDMS/ glass slide
And it is attached on SiO2On/Si substrate, MnB is obtained2- WSe2Heterojunction structure.
Tungsten source employed in the present embodiment and selenium source purity are 99.9% or more, the SiO of selection2/ Si substrate surface
Smooth and oxidated layer thickness is 285nm.
Although the present invention is disclosed as above with preferred embodiment, however, it is not intended to limit the invention.It is any to be familiar with
Those skilled in the art, without deviating from the scope of the technical scheme of the present invention, the method that may be by the disclosure above
Many possible changes and modifications are made to technical solution of the present invention with technology contents, or are revised as the equivalent reality of equivalent variations
Apply example.Therefore, anything that does not depart from the technical scheme of the invention according to the technical essence of the invention do above embodiments
Any simple modifications, equivalents, and modifications, belong to technical solution of the present invention protection in the range of.
Claims (10)
1. a kind of regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic, it is characterised in that including walking as follows
It is rapid:
(1) two-dimension single layer Transition-metal dichalcogenide is grown in substrate using chemical vapour deposition technique；
(2) two-dimentional feeromagnetic metal is prepared using mechanical stripping method；
(3) by alignment transfer platform, by two-dimentional feeromagnetic metal, alignment is transferred to two-dimension single layer Transition-metal dichalcogenide
On, form two-dimension single layer Transition-metal dichalcogenide-two dimension feeromagnetic metal heterojunction structure；Angle when by alignment transfer
Control realizes way of stacking different between two-dimension single layer Transition-metal dichalcogenide and two-dimentional feeromagnetic metal, to regulate and control two
Tie up the energy valley polarization characteristic of single layer Transition-metal dichalcogenide.
2. the regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic according to claim 1, feature
Be: the Transition-metal dichalcogenide molecular formula is MX2, M=Mo or W, X=S or Se.
3. the regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic according to claim 2, feature
Be: the Transition-metal dichalcogenide is tungsten disulfide, and step (1) is specifically: use tungstic acid and sulphur powder as
Chemical vapour deposition reaction source tips upside down on substrate on the quartz boat for being placed in reaction chamber middle storage tungstic acid, sulphur powder
It is placed in quartz boat and is placed at reaction chamber uptake, control reaction temperature and reaction time, deposition is grown in substrate, formed
Tungsten disulfide film.
4. the regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic according to claim 1 or 3, special
Sign is: the substrate is SiO2/ Si substrate.
5. the regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic according to claim 4, feature
Be: the substrate is prepared with the following method: by SiO2/ Si substrate is rinsed with a large amount of deionized waters, is successively put into acetone
It is cleaned by ultrasonic 5~10min in solution, ethanol solution and deionized water solution, cleaning is completed to take out substrate three times, and use is lazy
Property gas drying.
6. the regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic according to claim 5, feature
Be: the inert gas is nitrogen.
7. the regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic according to claim 1, feature
Be: step (2) is specifically: lower two-dimentional feeromagnetic metal is removed from feeromagnetic metal crystal using high transparency adhesive tape is thought, by adhesive tape
Repeatedly to gluing 5~8 times, two-dimentional feeromagnetic metal thin layer is obtained；Then it is adhered to and has been stained on the clean slide of PDMS, gently
Adhesive tape is taken off after micro- extruding 3~5 is lower.
8. the regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic according to claim 1 or claim 7, special
Sign is: the feeromagnetic metal is MnB2Or FeB2Or CrB2。
9. the regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic according to claim 1, feature
Be: step (3) is specifically: will grow the SiO for having single layer two dimension Transition-metal dichalcogenide2/ Si substrate is placed in pair
On quasi- transfer platform objective table, by being directed at transfer station, obtained two-dimentional feeromagnetic metal thin layer/PDMS/ glass slide is attached to
On single layer two dimension Transition-metal dichalcogenide, intermediate air is squeezed, two-dimentional feeromagnetic metal thin layer and single layer two dimension mistake are made
It crosses metal chalcogenide compound and pastes 10~20min of holding completely；Will sample place warm table on, at 60~80 DEG C heat 10~
After 30min, lower SiO is prized with tweezers low force2/ Si substrate makes hetero-junctions and PDMS/ glass slide be detached from and be attached on SiO2/ Si substrate
On；The two-dimension single layer transition gold of different way of stacking can be obtained in angles and positions control when by alignment transfer platform adherency
Belong to chalcogenide-two dimension feeromagnetic metal heterojunction structure.
10. the regulation method of two dimension Transition-metal dichalcogenide energy valley polarization characteristic according to claim 2, feature
It is that step (1) is specifically:
(a) first by SiO2/ Si substrate is cleaned with deionized water, and 5~10min is then cleaned by ultrasonic in acetone soln, is taken
Substrate is cleaned by ultrasonic 5~10min in being put into ethanol solution out, take out again substrate be put into deionized water cleaning 5~
10min, the SiO that cleaning is completed2/ Si substrate is with being dried with nitrogen；
(b) by SiO2It is indoor that/Si substrate and tungstic acid or molybdenum trioxide target source material are respectively put into thermal evaporation plated film instrument chamber
On luggage carrier and in crucible, chamber is evacuated to 10-4Pa using pumped vacuum systems, the target source material in heating crucible,
Its molecule is escaped from surface to form steam stream and deposit to SiO2/ Si substrate surface forms the raw material film of 1~5nm thickness；
(c) it is purged by pipe reaction stove evacuation to 10-2Torr, and with the argon gas of 200sccm to normal using pumped vacuum systems
Source material film/SiO of 0.5~10nm thickness will be deposited in pressure condition2/ Si substrate, which is put into quartz boat, is placed in tubular type
Then the heating zone center of furnace reaction chamber will grow the SiO of two-dimensional material2/ Si substrate is buckled to above this substrate, is protected
It holds between the two away from less than 1mm；
(d) it weighs 200mg sulphur powder or selenium powder is put into quartz boat and is placed at the uptake of reaction chamber, with quartz in (c)
The distance between boat is maintained between 10~20cm；
(e) it is maintained at the temperature of tube furnace reaction chamber central area between 600~950 DEG C by heating coil, sulphur or selenium
The temperature in source is maintained between 150~300 DEG C；Keep argon stream amount between 10~150sccm, growth time be 5~
60min；After growth is completed, heating coil is closed, is naturally cooling to room temperature in an argon atmosphere, takes out sample.
Priority Applications (1)
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